摘要: |
【目的】建立鸡血浆、肌肉、肝脏、肾脏中泰拉霉素残留的高效液相色谱 串联质谱(HPLC-MS/MS)检测方法。【方法】制备鸡血浆、肌肉、肝脏、肾脏泰拉霉素加标样品,经乙腈提取,SCX固相萃取小柱净化后,40 ℃氮气吹干,用乙腈-1 mL/L甲酸水溶液(体积比为1∶1)定容,Luna C18(2)色谱柱分离,以乙腈-1 mL/L甲酸水溶液(体积比为90∶10)为流动相进行梯度洗脱,通过质谱分析进行外标法定量,再通过试验确定HPLC MS/MS的检出限和定量限,并对血浆和肌肉、肝脏、肾脏分别进行10,20,50 μg/L 和10,20,50 μg/kg 3个水平的泰拉霉素添加回收试验。【结果】在5~200 μg/L血浆样品和 5~200 μg/kg肌肉、肝脏、肾脏样品中,泰拉霉素含量与峰面积呈良好的线性关系(R>0.99),血浆和肌肉、肝脏、肾脏样品中的泰拉霉素检出限依次为0.8 μg/L和0.5,0.8,0.5 μg/kg,定量限依次为2.0 μg/L和1.0,2.0,1.0 μg/kg。添加回收试验的平均回收率为80.3%~104.4%,日内相对标准偏差为5.0%~9.2%,日间相对标准偏差为5.2%~12.7%。【结论】HPLC-MS/MS方法简便、快速、准确,可用于鸡组织中泰拉霉素药物残留的确证和定量检测。 |
关键词: 鸡 泰拉霉素 残留检测 高效液相色谱 串联质谱法 |
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基金项目:安徽省高校省级自然科学基金重点项目(KJ2012A115) |
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Determination of Tulathromycin residues in chicken using liquid chromatography-tandem mass spectrometry |
XU Caoyan,LI Lin,TANG Chunlian,et al
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Abstract: |
【Objective】An analytical method based on liquid chromatography tandem mass spectrometry was developed for the determination of Tulathromycin residues in chicken tissues.【Method】Samples were extracted with acetonitrile and cleaned-up SCX cartridge.The Tulathromycin were separated with luna C18 column by a gradient elution program with 1 mL/L acetonitrile and 1 mL/L formic acid-water as the mobile phase.The identification of Tulathromycin was carried out by positive electrospray ionization (ESI+) in multiple-reaction monitoring (MRM) mode.The quantitation was performed by the external standard method.Add and recovery experiment was also conducted with different Tulathromycin levels for plasma,muscle,liver and kidney.【Result】There was a good linear relationship between Tara kanamycin concentration and peak area (R>0.99) in plasma (5-200 μg/L) and muscle,liver,and kidney (5-200 μg/kg).Recovery rates were 80.3% to 104.4% at three spiked levels of 10,20,50 μg/kg and the relative standard deviations (RSDs) were 5.0%-9.2% for intra-day and 5.2%-12.7% for inter-day determinations.Limit of detection (LOD) and limit of quantitation (LOQ) of plasma,muscle,liver,and kidney samples were 0.8 μg/L and 0.5,0.8,0.5 μg/kg,and 2.0 μg/L and 1.0,2.0,1.0 μg/kg,respectively.【Conclusion】The established method was simple,rapid,accurate and suitable for quantitative determination and confirmation of tulathromycin in real samples. |
Key words: chicken Tulathromycin residue detection high performance liquid chromatography tandem mass spectrometry (HPLC-MS/MS) |